Title: | Measurement of 18 perfluorinated organic acids and amides in human serum using on-line solid-phase extraction |
Author(s): | Kuklenyik Z; Needham LL; Calafat AM; |
Address: | "Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, Atlanta, Georgia 30341, USA. ZKuklenyik@cdc.gov" |
ISSN/ISBN: | 0003-2700 (Print) 0003-2700 (Linking) |
Abstract: | "We have developed an on-line solid-phase extraction (SPE) method coupled to high-performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) for measuring trace levels of 18 perfluorinated chemicals (3 perfluorosulfonates, 8 perfluorocarboxylates, 7 perfluorosulfonamides) in serum. Without protein precipitation, only dilution with 0.1 M formic acid, one aliquot of 100 microL of serum was injected into a commercial column switching system that allowed for concurrent SPE and HPLC-MS/MS acquisition. First, the analytes were concentrated on a C18 SPE column. Then, this column was placed automatically in front of a C8 analytic HPLC column for chromatographic separation of the analytes. Detection and quantification were done using negative-ion TurboIonSpray ionization, a variant of electrospray ionization, MS/MS. Excellent recovery was achieved for all analytes including the volatile sulfonamide derivatives that could not be determined before using traditional off-line SPE methods. The high throughput and low limits of detection (0.05-0.8 ng/mL) using a small sample volume (100 microL of serum) and isotope dilution quantification make this method suitable for large-scale epidemiologic studies" |
Keywords: | "Acids/chemistry Amides/*blood/chemistry Chromatography, High Pressure Liquid Fluorine Compounds/*blood/chemistry Humans Online Systems/*instrumentation Organic Chemicals/*blood/chemistry Solid Phase Extraction/*instrumentation/*methods Tandem Mass Spectro;" |
Notes: | "MedlineKuklenyik, Zsuzsanna Needham, Larry L Calafat, Antonia M eng 2005/09/15 Anal Chem. 2005 Sep 15; 77(18):6085-91. doi: 10.1021/ac050671l" |